US10978279B2 - Tubular target having a protective device - Google Patents

Tubular target having a protective device Download PDF

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Publication number
US10978279B2
US10978279B2 US14/110,527 US201214110527A US10978279B2 US 10978279 B2 US10978279 B2 US 10978279B2 US 201214110527 A US201214110527 A US 201214110527A US 10978279 B2 US10978279 B2 US 10978279B2
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Prior art keywords
tubular target
protective device
molybdenum
cooling medium
tubular
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US20140027276A1 (en
Inventor
Christian Linke
Manfred Sulik
Martin Kathrein
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Plansee SE
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Plansee SE
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/342—Hollow targets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491—Manufacturing of targets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3497—Temperature of target

Definitions

  • the invention relates to a tubular target for cathode atomization which has no backing tube and is made of molybdenum or a molybdenum alloy with a molybdenum content of at least 50 at. %, having a sputtering surface and an inner surface which is in contact at least in certain regions with a cooling medium.
  • Tubular targets made of pure molybdenum and molybdenum alloys, for example Mo—Na are used for the deposition of Mo-containing layers by cathode atomization, for example magnetron sputtering, including during the production of thin-film solar cells based on Cu(In x ,Ga 1-x )(Se y ,S 1-y ) 2 (with Ga:CIGS, without Ga:CIS) or thin-film transistors for TFT-LCD.
  • the Mo-containing layers in this case have thicknesses of a few nm up to a few ⁇ m.
  • sputtering targets The starting materials required for sputtering (cathodes) are referred to as sputtering targets and, depending on the design of the coating systems, can be used with a planar or tubular geometry.
  • tubular sputtering targets also called tubular targets, are rotated about a stationary or moving magnetic system arranged in the interior of the target.
  • tubular sputtering targets Compared with planar sputtering targets, tubular sputtering targets have the advantage that uniform removal of the material and therefore a higher material yield are achieved.
  • Tubular sputtering targets have gained acceptance particularly for expensive materials with complex production.
  • the tubular target is formed at least in two parts so as not to allow the forces which are required for holding and moving the tubular target to act on the brittle and therefore breakable sputtering material.
  • a tube or a plurality of tube segments made of the sputtering material are joined to a backing tube, made for example of a non-magnetic steel or titanium.
  • a backing tube made for example of a non-magnetic steel or titanium.
  • soldering processes using low-melting solders for example indium or indium alloys.
  • More than 75% of the energy introduced during sputtering is introduced as heat into the sputtering target.
  • the thermal energy which is produced by the bombardment with high-energy ions on the surface of the sputtering target has to be dissipated in a sufficiently effective manner so as to prevent the sputtering target and/or the soldering material from overheating.
  • the cooling of the sputtering targets is therefore of decisive importance.
  • the inner surface of the sputtering target is cooled over the entire surface area or in certain regions by a cooling medium which flows through. In this case, depending on the design of the tubular targets, the cooling medium is in direct contact either with the sputtering material or the backing tube.
  • Tubular targets made of molybdenum or a molybdenum alloy are commonly used with a backing tube.
  • This has the disadvantage not only of the complex joining of sputtering material and backing tube but also of the dissipation of heat which is hindered by the solid backing tube and soldering material.
  • steels have considerably poorer heat conduction properties than molybdenum.
  • a tubular target made of molybdenum or a molybdenum alloy is formed without a backing tube, there is direct contact between the cooling medium and the target material.
  • Molybdenum and molybdenum alloys corrode under the long-lasting action of conventional cooling media. In this case, the corrosion rate is up to a few 1/10 of a millimeter per year, depending on the composition and nature of the cooling medium and on the conditions of use.
  • the dissolution of the molybdenum caused by the contact with the cooling medium and the corrosion products which form in the process lead to a change in the properties of the cooling medium.
  • the pH value of the cooling medium can be lowered considerably and therefore the further materials which are used in the cooling circuit (such as copper, brass, high-grade steel) can be subjected to an increased corrosive attack.
  • the corrosion of the molybdenum and other materials in the cooling circuit can be reduced, but not completely avoided, by adding inhibitors on an organic or inorganic basis to the coolant. Corrosion inhibitors for molybdenum are described, for example, in U.S. Pat. No. 4,719,035 (A).
  • Cooling medium Distilled water, softened water, mains water Inlet temperature Approx. 20° C. Outlet temperature Approx. 25-40° C. pH value 7.5-9.5 Electrical conductance 100-2000 ⁇ S/cm Inhibitors Organic inhibitors, for example thiazoles, triazoles; inorganic inhibitors, for example molybdates Biocides Organic or inorganic broadband biocides
  • molybdenum tubular targets comprising a backing tube therefore firstly have to be desoldered and the soldering materials, which are conventionally of a different type for steel alloys, have to be removed in a complex manner.
  • the dissipation of heat has to be ensured to an adequate extent, that corrosion is avoided as far as possible throughout the service life of the tubular target and that used sputtering targets can easily be used as alloying material for the steel industry.
  • the object is achieved by the characterizing part of the independent claim.
  • the embodiment according to the invention reliably avoids corrosion and does not inadmissibly impair the dissipation of heat.
  • the used tubular targets can be used as alloying scrap for the production of steel without complex separation or cleaning, since the quantitative proportions of the protective device in terms of the molybdenum proportion are small.
  • the tubular target consists of pure molybdenum or a molybdenum alloy.
  • “molybdenum alloys” are understood to mean all Mo-containing materials with an Mo content of greater than 50 at. %. If molybdenum is mentioned hereinbelow, this always encompasses pure molybdenum and Mo-containing materials with an Mo content of greater than 50 at. %.
  • the tubular target is formed with no backing tube. In this case, “with no backing tube” means that no backing tube is used.
  • the molybdenum tubular target is therefore joined directly to the holding system of the sputtering system or to the end block.
  • the outer surface of the tubular target is designated as the sputtering surface.
  • the inner surface corresponds to the inner wall of the tubular target. At least one region of the inner surface is separated from the cooling medium by at least one protective device. There is advantageously areal contact between the target material and the protective device. Furthermore, it is preferable for all of the inner surface which is in contact with the cooling medium to be separated from the cooling medium by at least one protective device. It is advantageous if the protective device has a thickness (measured in the radial direction) of 0.0005 mm to 1 mm. It is particularly advantageous if the protective device has a thickness (measured in the radial direction) of 0.0005 mm to 0.1 mm.
  • the thermal conductivity of the protective device is less than 1 W/m ⁇ K, a thickness of the protective layer of 0.0005 mm to 0.5 mm is preferable. Furthermore, it is advantageous if the protective device is a single-ply or multi-ply layer. In order to improve the layer adhesion, it is advantageous to pretreat, e.g. to degrease or to roughen, the inner surface of the tube before the protective device is applied. Further advantageous embodiments are protective devices in the form of a thin-walled film or of a thin-walled tube which lie seamlessly against the inner surface of the tubular target each under the action of the pressurized coolant.
  • the protective device is understood in turn to mean thicknesses in the range of up to 1 mm.
  • the protective device is preferable for the protective device to consist at least of one material from the group consisting of polymer, metal, ceramic and glass.
  • An example of a suitable metal is nickel, which can be applied in a simple manner by chemical nickel plating.
  • nickel which can be applied in a simple manner by chemical nickel plating.
  • Mo nitride which can be produced in a simple manner by nitriding the Mo tube.
  • Systems based on silicon oxide are suitable in particular for layers of glass.
  • materials which have proved to be suitable are those which are noncritical for steel production, for example polymers, the constituents of which (carbon) firstly represent noncritical admixtures in terms of the overall carbon content of the steel, and secondly escape in gas form during steel production (nitrogen, hydrogen, chlorine, fluorine, . . . ). If the protective device consists of ceramic or glass, the constituents are deposited in the slag during steel production.
  • the protective device comprises at least one polymer. It is particularly advantageous if the polymer has a thermal conductivity of greater than 0.5 W/m ⁇ K, in particular greater than 1 W/m ⁇ K. Electrical conductivity also has an advantageous effect on the use properties of the tubular target. Thermal and/or electrical conductivity are achieved, for example, if the polymer is provided with one or more conductive fillers. Suitable fillers which can be mentioned are materials from the group consisting of ceramic, graphite and metal.
  • Particularly suitable fillers are Cu, Al, Si, Zn, Mo, W, oxides, for example Al 2 O 3 , nitrides, for example AlN, TiN, BN, MoN or SiN, carbides, for example SiC, TiC or WC, and graphite.
  • the protective device consists of at least one polymer.
  • Particularly suitable polymers are polymers from the group consisting of epoxy resin, polyethylene, polypropylene, polyurethane, polyvinyl chloride, polyester, vinyl ester and fluoroelastomer.
  • the protective device can advantageously be applied or introduced by means of wet coating, painting, spraying or insertion of a film.
  • CVD chemical vapour deposition
  • PVD cathode atomization
  • galvanizing chemical and electrochemical processes, sintering, diffusion coating, rubbing or back-casting.
  • the FIGURE shows an oblique view of the tubular target - 1 - according to the invention having a sputtering surface - 2 -, and inner surface - 3 - and a protective device - 4 -.
  • a molybdenum tube - 1 - having an internal diameter of 125 mm, an external diameter of 165 mm and a sputtering surface - 2 - was produced in accordance with the process described in EP 1 937 866 (A).
  • the inner surface - 3 - of the molybdenum tube which was to be coated had a length of 1500 mm.
  • the turned inner surface was firstly roughened by sand blasting.
  • the subsequent coating was effected by brushing on an epoxy resin filled with 70% by volume Al having a particle size of 50 ⁇ m.
  • the layer thickness of the protective device - 4 - was approximately 300 ⁇ m.
  • Cylindrical molybdenum samples having a diameter of 10 mm and a length of 50 mm were tested for corrosion resistance in the uncoated and coated (Examples 2a to 2g) state in exposure tests.
  • the samples were stored in various cooling media over a period of time of 160 hours, and the loss in mass of the samples was measured.
  • the coolant bath was agitated by means of a magnetic stirrer during the test period.
  • the results of the measurements are shown in Table 2.
  • the samples designated with R correspond to the prior art (uncoated).
  • Examples 2a to 2g are examples according to the invention.
  • the turned surface was roughened by sand blasting.
  • the subsequent coating was effected by brushing on an epoxy resin comprising 70% by volume Al having a particle size of 50 ⁇ m.
  • the layer thickness was approximately 300 ⁇ m.
  • the turned surface was roughened by sand blasting.
  • the subsequent coating was effected by wet coating with an alkyd resin paint (a polyester), which was dried out in air.
  • the layer thickness was approximately 100 ⁇ m.
  • the turned surface was roughened by sand blasting.
  • the subsequent coating was effected by brushing on an epoxy resin filled with 70% by volume Al 2 O 3 .
  • the layer thickness was approximately 300 ⁇ m.
  • the turned surface was cleaned and degreased by pickling.
  • the subsequent coating was effected by means of the powder spraying of a polyurethane compound.
  • the layer thickness was approximately 500 ⁇ m.
  • the turned surface was cleaned and degreased by pickling.
  • a layer of copper having a thickness of 15 ⁇ m was deposited by a conventional electrochemical process (copper sulphate basis).
  • the turned surface was roughened by sand blasting.
  • An SiO 2 -based slurry was then applied and heat-treated at 200° C./60 min.
  • the turned surface was roughened by sand blasting.
  • a TiN layer having a thickness of 2 ⁇ m was then applied by means of CVD.
US14/110,527 2011-04-08 2012-04-05 Tubular target having a protective device Active 2033-03-21 US10978279B2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
ATGM203/2011U AT12695U1 (de) 2011-04-08 2011-04-08 Rohrtarget mit schutzvorrichtung
ATGM203/2011U 2011-04-08
ATGM203/2011 2011-04-08
PCT/AT2012/000094 WO2012135883A1 (de) 2011-04-08 2012-04-05 Rohrtarget mit schutzvorrichtung

Publications (2)

Publication Number Publication Date
US20140027276A1 US20140027276A1 (en) 2014-01-30
US10978279B2 true US10978279B2 (en) 2021-04-13

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US14/110,527 Active 2033-03-21 US10978279B2 (en) 2011-04-08 2012-04-05 Tubular target having a protective device

Country Status (8)

Country Link
US (1) US10978279B2 (de)
EP (1) EP2694697B1 (de)
JP (1) JP6328550B2 (de)
KR (1) KR102068366B1 (de)
CN (2) CN103518002A (de)
AT (1) AT12695U1 (de)
TW (1) TWI568870B (de)
WO (1) WO2012135883A1 (de)

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US9992917B2 (en) 2014-03-10 2018-06-05 Vulcan GMS 3-D printing method for producing tungsten-based shielding parts
CN105296944A (zh) * 2015-10-27 2016-02-03 有研亿金新材料有限公司 一种具有抗氧化镀层的靶材组件
TW201911853A (zh) * 2017-08-10 2019-03-16 聚晶半導體股份有限公司 雙攝像頭影像擷取裝置及其攝像方法
CN108517498B (zh) * 2018-04-17 2020-04-21 洛阳科威钨钼有限公司 一种用于磁控溅射的一体式管状钼靶材的制备方法

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